CN104761659B - Method for preparing butyl rubber solution for halogenation, and apparatus thereof - Google Patents
Method for preparing butyl rubber solution for halogenation, and apparatus thereof Download PDFInfo
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- CN104761659B CN104761659B CN201410003515.7A CN201410003515A CN104761659B CN 104761659 B CN104761659 B CN 104761659B CN 201410003515 A CN201410003515 A CN 201410003515A CN 104761659 B CN104761659 B CN 104761659B
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Abstract
The invention discloses a method for preparing a butyl rubber solution for halogenations. The method comprises the following steps: 1, allowing a butyl rubber slurry to contact with hexane steam in a flash evaporation kettle to obtain a gas phase product and a hexane solution of butyl rubber; and 2, directly introducing the hexane solution of butyl rubber obtained in step 1 into a guide sieve tray tower, and allowing the hexane solution of butyl rubber to contact with the hexane steam in a countercurrent manner in order to directly obtain the butyl rubber hexane solution for halogenation. The method allows the rubber solution for halogenation to be directly obtained by removing unreacted monomers residual in the hexane solution of butyl rubber through the high efficiency guide sieve tray tower, so the production flow of halogenated butyl products is simplified, and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of method preparing butyl rubber solution, more particularly, to a kind of halogenation butyl rubber
The preparation method of hexane solution.
Background technology
Halogenated butyl rubber（HIIR）On the basis of keeping the original performance of butyl rubber, fast with curingprocess rate, Ke Yiyu
General purpose resilient body co-vulcanization, adhesive property is good, becomes production tubeless meridian wheel the features such as have more preferable heat resistance
The preferred material of tire inner liner.The production technology of halogenated butyl rubber is mainly carried out using solwution method at present, that is, adopt saturation alkane
Hydrocarbon（As hexane）Obtain certain density glue for solvent dissolving butyl rubber, then carry out halogenation.Solwution method halobutyl
The production process of rubber includes three parts：（1）The production of basic butyl rubber；（2）Glue carries out halogenation；（3）Product
Cohesion drying.Different companies, because production technology level is different, the technical process being adopted and process detail also each not
Identical, wherein main difference concentrates in glue preparation technology.For glue preparation technology, then there are the poly- sol method of water-setting and oneself
Alkane strips sol method.Generally, can be used in the glue of halogenation（Butyl rubber hexane solution）It is desirable to butyl rubber
Content is 10-20wt%, and the content of unreacted monomer is low.But prior art does not reach the gelatin concentration of regulation, therefore, it is necessary to
Follow-up concentration is carried out to glue, just can access the glue for halogenation.
The poly- sol method of water-setting is to first pass through water steam stripping coacervation and obtain micelle aqueous slurry to dehydrate and then use hexane colloidal sol
Form glue.Higher using water content in the glue of this method preparation, and cannot thoroughly remove, therefore to follow-up halogenation mistake
Journey impact is larger, does not only result in bromine utilization rate and declines, more seriously equipment corrosion excessive velocities, thus cause device unplanned
Stop or stop production, affect product quality and production efficiency.
Document is had to disclose one kind using unreacted monomer and solvent one chloromethane in hot hexane stripping butyl rubber slurry
Alkane, the method continuously producing halogenation use or preparing the glue of latex, i.e. hexane stripping sol method.This method includes：Will
The butyl rubber slurry being formed is passed through flash vaporization kettle, and overheated hexane is also passed into flash vaporization kettle in vapour form simultaneously, and hexane vapor discharges
Go out enough heat most monochloro methanes of gasification and unreacted monomer, butyl rubber rapidly dissolves shape in hexane simultaneously
Become hexane solution, be dissolved with butyl rubber hexane solution enter glue stripper top, glue to bottom of towe flow while and
The hexane vapor contact that adverse current rises carries out mass transfer, to remove the unsaturated monomer of residual in glue.It is substantially free of alkene list
The butyl rubber hexane solution of body is discharged from stripper bottom, enters the second flash vaporization kettle.In the second flash vaporization kettle, part hexane steams
Send out the gelatin concentration making butyl rubber solution be concentrated into regulation, the butyl rubber solution after then concentrating is used for follow-up reaction,
As halogenation.Whole technological equipment investment is high, technological process is long.
Remain a need for process is simple and can in efficient removal butyl rubber solution unreacted monomer to prepare halogenation butyl rubber
The method of sol solution.
Content of the invention
In view of above-mentioned prior art situation, present inventor is carried out in rubber materials and chemical industry rectification and purification field
A kind of research extensively and profoundly, there is provided unreacted monomer in process is simple and energy efficient removal butyl rubber solution, directly
To high concentration（10-20wt%）Butyl rubber hexane solution method, directly obtain can be used for halogenation butyl rubber oneself
Alkane solution.
According to an aspect of the invention, it is provided a kind of method preparing halogenation butyl rubber solution, it includes：
Butyl rubber slurry is contacted in flash vaporization kettle by step i. with hexane steam, and the hexane obtaining containing butyl rubber is molten
Liquid,
The hexane solution of the butyl rubber obtaining in step i is passed directly into guide sieve-plate tower by step ii., in linde sieve tray
Inversely contact with hexane steam in tower, directly obtain the butyl rubber hexane solution that can be used for halogenation.
In a specific embodiment of the method for the invention, the butyl rubber hexane solution that obtains in described step ii
Middle butyl rubber content is 10-20wt%.In another is embodied as, the hexane of the butyl rubber obtaining in described step ii
In solution, unreacted monomer content is less than 1ppm.
According to method of the present invention, the flash vaporization kettle kettle top in described step i obtains gas-phase product, and wherein, gas phase is produced
Thing includes unreacted monomer, alkyl halide diluent and hexane.
According to a preferred embodiment of the method for the invention, the charging position that butyl rubber slurry is passed through flash vaporization kettle is high
Charging position in hexane steam.As hexane can be passed through in the bottom of flash vaporization kettle, butyl rubber slurry is led on the top of flash vaporization kettle
Enter.
According to another preferred embodiment of the method for the invention, the hexane containing butyl rubber obtaining in step i is molten
The charging position that liquid is passed through guide sieve-plate tower is higher than the charging position of hexane steam.As hexane can lead in the bottom of guide sieve-plate tower
Enter, the hexane solution containing butyl rubber is passed through on the top of guide sieve-plate tower.
According to method of the present invention, the operation temperature of described flash vaporization kettle is 30-70 DEG C, and operating pressure is 0.1-
0.5MPa.The temperature of described guide sieve-plate tower is 30-150 DEG C, preferably 50-90 DEG C；Pressure is 5-500KPa, preferably 20-
200KPa.
The method being provided according to the present invention, overcomes deficiency of the prior art, by flash vaporization kettle plus guide sieve-plate tower
Combination is it is possible to directly obtain the butyl rubber hexane solution that concentration is 10-20wt%, it is anti-that described solution can be directly used for halogenation
Should, and need not other concentration steps, simplify the technological process of production, reduce equipment investment, reduce production cost, improve
Economic benefit.
According to another aspect of the present invention, there is provided it is molten that a kind of profit prepares halogenation butyl rubber with the aforedescribed process
The device of liquid, including：
Flash vaporization kettle,
The guide sieve-plate tower being joined directly together with flash vaporization kettle.
The device being provided according to the present invention, the butyl rubber hexane solution obtaining from guide sieve-plate tower bottom of towe can be directly used for
Halogenation.
According to a specific embodiment of device of the present invention, the butyl directly obtaining from described linde sieve tray tower bottom
In rubber hexane solution, butyl rubber concentration is 10-20wt%.In another instantiation, from described linde sieve tray tower bottom
In the butyl rubber hexane solution directly obtaining, unreacted monomer content is less than 1ppm.
Some connecting pipes are also included according to device of the present invention, does not elaborate again herein.Described have at one
In body example, the operation temperature of flash vaporization kettle is 30-70 DEG C, and operating pressure is 0.1-0.5MPa.The temperature of described guide sieve-plate tower
For 30-150 DEG C, preferably 50-90 DEG C；Pressure is 5-500KPa, preferably 20-200KPa.
The method and apparatus being provided using the present invention, butyl rubber slurry is passed through flash vaporization kettle, overheated hexane is to steam simultaneously
Gas form is also passed into flash vaporization kettle, the heat most alkyl halide diluent of gasification being discharged using hexane vapor（As a chloromethane
Alkane）And unreacted monomer, simultaneously butyl rubber rapidly dissolve in hexane formation hexane solution.Butyl rubber will be dissolved with
Hexane solution passes through pump or relies on pressure reduction to send into high-efficiency guide sieve-plate tower, removes the unreacted monomer of residual and alkyl halide in glue
Diluent（As monochloro methane）.Obtain is substantially free of unreacted monomer and the butyl rubber hexane solution for 10-20% for the concentration
Directly carry out halogenation.
The method and apparatus being provided according to the present invention, is removed using guide sieve-plate tower in the hexane solution of butyl rubber not
Reaction monomers, not only plate pressure drop is low, efficiency high, it is possible to achieve energy-saving, and is particularly well-suited to high viscous material, Ke Yiyou
Effect overcomes the defects such as stifled tower, liquid flooding, entrainment so that the unreacted list in butyl rubber solution substantially can be removed completely
Body and monochloro methane, the solution that bottom of towe obtains can directly carry out halogenation.
The method and apparatus being provided according to the present invention, butyl rubber slurry is passed through flash vaporization kettle, is inversely connect with hexane steam
Touch and mass transfer, remove the most of unreacted monomer in butyl rubber slurry and alkyl halide diluent, the butyl in slurry simultaneously
Rubber is rapidly dissolved in hexane, obtains the hexane solution containing butyl rubber, meanwhile, from flash vaporization kettle out containing butyl rubber oneself
Alkane solution still contains unreacted monomer and alkyl halide diluent；Hexane solution containing butyl rubber is passed directly into linde sieve tray
Tower, using the structure of guide sieve-plate tower, can except vanishing viscosity contain in the hexane solution of butyl rubber the unreacted monomer of residual and
Monochloro methane so that in the hexane solution of butyl rubber that obtains of bottom of towe the content of unreacted monomer can be reduced to 1ppm with
Under, the concentration of the hexane solution of butyl rubber is sufficiently high simultaneously, such as 10-20%, can directly carry out halogenation.
The method according to the invention and device, the hexane that can directly obtain the butyl rubber that can carry out halogenation is molten
Liquid, and the step of other processing solutions that need not be extra.Compare with prior art, technological process is simple, and can efficient removal fourth
Unreacted monomer in base rubber solutions, reduces energy consumption and material consumption；Simplify the production procedure of halobutyl, reduce production
Cost.
These and other purposes, features and advantages of the present invention, will be easily after integrally considering the present invention with reference to drawings described below
In being understood by those of ordinary skill.
Brief description
Fig. 1 be according to one embodiment of the present of invention process chart.
Specific embodiment
In embodiments of the present invention, step i. is passed through using the butyl rubber slurry that such as slurry polymerization obtains
Flash vaporization kettle, simultaneously overheated hexane be also passed into flash vaporization kettle in vapour form, the heat gasification being discharged using hexane vapor is most of
Monochloro methane and unreacted monomer, simultaneously butyl rubber rapidly dissolve in hexane formation hexane solution；Step ii. is then
The hexane solution of butyl rubber will be dissolved with as pressure reduction can be relied on to send into guide sieve-plate tower（Preferably employ high-efficiency guide sieve-plate tower）,
It is passed through hexane vapor from bottom of towe simultaneously, make glue and hexane vapor counter current contacting carry out mass transfer, in removing solution, residual is not anti-
Answer monomer and monochloro methane.Finally unreacted monomer content is less than 1ppm and concentration is the butyl rubber hexane of 10-20wt%
Solution directly carries out halogenation.
In the another embodiment of the inventive method, the butyl rubber slurry that step i. is obtained using such as slurry polymerization
It is passed through flash vaporization kettle, overheated hexane is also passed into flash vaporization kettle in vapour form simultaneously, the heat gasification discharging using hexane vapor is big
Partial monochloro methane and unreacted monomer, simultaneously butyl rubber rapidly dissolve in hexane formation hexane solution；Step ii.
Then the hexane solution of butyl rubber will be dissolved with by being pumped into efficient sieve plate tower, remove the unreacted monomer of residual in glue
And monochloro methane.Finally unreacted monomer content is less than 1ppm and the butyl rubber hexane solution for 10-20wt% for the concentration is straight
Tap into row halogenation.
The term being used in the context of the present invention " butyl rubber " should be understood to refer to the isomery that carbon number is 4-8
Alkene, such as isobutene, and carbon number is the conjugated diene of 4-8, such as the copolymer of isoprene.The matter of wherein isomeric olefine
Amount fraction is 60-99.5%, and the mass fraction of conjugated diene is 40-0.5%.Unreacted monomer in the present invention is it is simply that refer to carbon
Atomicity is the isomeric olefine of 4-8, and such as isobutene, and carbon number is the conjugated diene of 4-8, such as isoprene.Butyl rubber
The production of glue generally adopts slurry process, with halogenated alkane as diluent, such as monochloro methane, reaction temperature control -90 DEG C～-
107℃.
Butyl rubber slurry in the present invention refers to halogenated alkane as diluent, the isomery alkene with carbon number as 4-8
Hydrocarbon and the conjugated diene that carbon number is 4-8 are monomer, the polymer slurries being obtained using slurry polymerization.
It is necessary to first butyl rubber is dissolved in formation solution in varsol before halogenating butyl rubber.According to the present invention
The method providing, can directly obtain the glue of halogenation.Compared with sol method poly- with water-setting, not only eliminate basic butyl
Rubber micelle aqueous slurry dehydration drying system, also due to there is not the circulation of water in system and eliminate being dried of monochloro methane be
System, production technology is simplified.
A small amount of unreacted monomer and monochloro methane is also remained in the butyl rubber hexane solution being formed in flash vaporization kettle,
Need to be removed, otherwise remaining in the monomer in glue can be reacted formation halide with halogen.These halide are final
Can remain in the product, not only affect the content of halogen index of product, and especially bromide can become dacryagogue, to rear place
Reason packaging and mixed refining process cause compared with burden.
By the butyl rubber hexane solution remaining a small amount of unreacted monomer and monochloro methane is passed through guide sieve-plate tower,
Viscous glue solution can be removed（Or claim the hexane solution of butyl rubber）The unreacted monomer of middle residual and monochloro methane.（Efficiently）Lead
Refer to the document of Lie group life etc. to the concrete structure of sieve-plate tower：High-efficiency guide sieve-plate tower removes VAc monomer rectifying to PVAc
Technological transformation, chemical industry is in progress, 2011, volume 30 supplementary issue, the 783-786 page.The column plate of high-efficiency guide sieve-plate tower has
A number of pilot hole, makes the gas front progradation oriented to liquid plate spraying from guiding hole horizontal, effectively disappears
Except gradient of liquid level and backmixing of liquid phase.On the other hand, the raised bubbling of sloping platform shape is set in the liquid-inlet area of column plate and promotes dress
Put, make liquid one enter column plate and be activated, cause the advantage of whole column plate bubbling, simultaneously effective reduce column plate pressure
Fall, improves plate efficiency.Using the favourable configurations of guide sieve-plate tower, enable to unreacted monomer in the glue that bottom of towe obtains
Content can be reduced to below 1ppm, and gelatin concentration is sufficiently high simultaneously, such as 10-20%, can directly carry out halogenation.
The present invention compared with prior art, mainly has following beneficial effect：
（1）Directly adopt hot hexane removing monochloro methane and unreacted monomer, the glue of halogenation can be directly obtained
Liquid, production technology is simplified.
（2）Remove unreacted monomer and the monochloro methane in glue, not only plate pressure drop using efficient guide sieve-plate tower
Low, efficiency high, it is possible to achieve energy-saving, and it is particularly well-suited to high viscous material, can effectively overcome stifled tower, liquid flooding, mist
The defect such as carry secretly so that the concentration of solution can be up to 20wt% in tower, the glue that bottom of towe obtains directly can carry out halogenation,
Simplify the production process of halobutyl, reduce production cost.
Below in conjunction with accompanying drawing 1, the inventive method is described further.As shown in figure 1, the inventive method dress used
Put main inclusion flash vaporization kettle I and guide sieve-plate tower II.Equipped with agitator in flash vaporization kettle I.It should be understood that for clear mesh
, Fig. 1 is not provided with some parts or the details of device construction, because such details is conventional and is people in the art
Member is known.Additionally, in order to the present invention is explicitly described, also eliminating the conventional control of many chemical fields or detection in FIG
Device.
First, polymer slurries 1 are sent into flash vaporization kettle I.The temperature of flash vaporization kettle I is sufficiently high, with effective gasification alkyl halide
Diluent（As monochloro methane）.The operation temperature of flash vaporization kettle I at 30～70 DEG C, such as 55 DEG C, operating pressure be 0.1～0.5MPa it
Between, such as 0.14MPa, simultaneously overheated hexane vapor 2 also spray into flash vaporization kettle I.Hexane vapor discharges enough heat gasification one chlorine
Methane.Control the amount of vaporization of alkyl halide diluent (as monochloro methane) by adjusting the temperature and pressure of flash vaporization kettle I, make a large amount of
Alkyl halide diluent (as monochloro methane) gasification, about 70%～99%（As 90%）Alkyl halide diluent (as a chloromethane
Alkane) removed by evaporation, butyl rubber rapidly dissolves in hexane simultaneously.Gas-phase product 3（Alkyl halide diluent including gasification
(as monochloro methane) and unreacted monomer and part hexane）Flow out from kettle top, be dissolved with the hexane solution of butyl rubber simultaneously（Glue
Liquid）4 entrance（Efficiently）Guide sieve-plate tower II.Hexane vapor 2 ' enters from bottom of towe and flows up, and contacts with the glue 4 flowing downward
Carry out mass transfer, in glue, the unreacted monomer of residual and alkyl halide diluent (as monochloro methane) rise with hexane vapor, with gas
The form of phase product 5 flows out from tower top, and bottom of towe obtains the butyl rubber hexane solution 6 that unreacted monomer content is less than 1ppm, fourth
Base rubber hexane solution 6 concentration is 10-20%.The temperature of high-efficiency guide sieve-plate tower II should control will not make depolymerization, lead to
Often it is less than 150 DEG C, operating pressure is 5-500KPa.
Below with reference to embodiment, the present invention is specifically described, but described embodiment is not to scope of the invention structure
Become any restriction.
Embodiment 1
The butyl rubber slurry obtaining using slurry polymerization is passed through the flash vaporization kettle that volume is 120m3, butyl rubber becomes silted up
The inlet amount of slurry is 21681.3kg/h, consists of：Monochloro methane 77.0%, butyl rubber 18.4%, isobutene 4.4%, isoamyl two
Alkene 0.2%.150 DEG C of overheated hexane vapor is also passed into flash vaporization kettle.Carry out flash distillation under 55 DEG C, 0.13MPa, monochloro methane
Amount of vaporization is 92%, and under stirring, butyl rubber dissolving forms glue in hexane, and the flow of glue is 43961.5kg/
H, consists of hexane 87.5%, monochloro methane 3.1%, butyl rubber 9.1%, isobutene 0.3%, isoprene 353ppm.In pressure reduction
In the presence of, glue enters the top of high-efficiency guide sieve-plate tower, and bottom of towe is passed through 150 DEG C of overheated hexane vapor, and high-efficiency guide sieves
15 pieces of the number of theoretical plate of plate tower, feeds at the 3rd piece.The material composition of the operating condition of tower and tower top, bottom of towe is shown in Table 1 and table respectively
2.In glue, the content of isoprene is 0.8ppm, and gelatin concentration is 10%.The glue that bottom of towe obtains directly carries out halogenation.
The operating condition of table 1 high-efficiency guide sieve-plate tower
Table 2 tower top and materials at bottom of tower composition
Embodiment 2
The butyl rubber slurry obtaining using slurry polymerization is passed through the flash vaporization kettle that volume is 120m3, butyl rubber becomes silted up
The inlet amount of slurry is 21681.3kg/h, consists of：Monochloro methane 77.0%, butyl rubber 18.4%, isobutene 4.4%, isoamyl two
Alkene 0.2%.150 DEG C of overheated hexane vapor is also passed into flash vaporization kettle.Carry out flash distillation under 40 DEG C, 0.13MPa, monochloro methane
Amount of vaporization is 75%, and under stirring, butyl rubber dissolving forms glue in hexane, and the flow of glue is 64152.8kg/
H, consists of hexane 86.6%, monochloro methane 6.5%, butyl rubber 6.2%, isobutene 0.6%, isoprene 485ppm.Will with pump
Glue sends into high-efficiency guide sieve-plate tower, 14 pieces of the number of theoretical plate of guide sieve-plate tower, feeds at the 5th piece.The operating condition of tower and tower
Top, the material composition of bottom of towe are shown in Tables 1 and 2 respectively.In glue, the content of isoprene is 0.11ppm, and gelatin concentration is 15%.
The glue that bottom of towe obtains directly carries out halogenation.
The operating condition of table 1 high-efficiency guide sieve-plate tower
Table 2 tower top and materials at bottom of tower composition
Embodiment 3
The butyl rubber slurry obtaining using slurry polymerization is passed through the flash vaporization kettle that volume is 120m3, butyl rubber becomes silted up
The inlet amount of slurry is 21681.3kg/h, consists of：Monochloro methane 77.0%, butyl rubber 18.4%, isobutene 4.4%, isoamyl two
Alkene 0.2%.150 DEG C of overheated hexane vapor is also passed into flash vaporization kettle.Carry out flash distillation under 70 DEG C, 0.25MPa, monochloro methane
Amount of vaporization is 82%, and under stirring, butyl rubber dissolving forms glue in hexane, and the flow of glue is 54277.0kg/
H, consists of hexane 86.8%, monochloro methane 5.3%, butyl rubber 7.4%, isobutene 0.5%, isoprene 432ppm.In pressure reduction
In the presence of, glue enters the top of high-efficiency guide sieve-plate tower, 10 pieces of the number of theoretical plate of high-efficiency guide sieve-plate tower, enters at the 3rd piece
Material.The material composition of the operating condition of tower and tower top, bottom of towe is shown in Tables 1 and 2 respectively.In glue, the content of isoprene is
0.3ppm, gelatin concentration is 20%.The glue that bottom of towe obtains directly carries out halogenation.
The operating condition of table 1 high-efficiency guide sieve-plate tower
Table 2 tower top and materials at bottom of tower composition
By data above it is known that the method being provided according to the present invention, can effectively remove in butyl rubber slurry
Unreacted monomer and alkyl halide diluent, in the hexane solution of the butyl rubber obtaining, the concentration of butyl rubber is high, unreacted list
The content of body is low, can be directly used for halogenation.
It should be noted that embodiment described above is only used for explaining the present invention, do not constitute any to the present invention
Limit.By referring to exemplary embodiments, invention has been described, it should be appreciated that word wherein used is descriptive
With explanatory vocabulary, rather than limited vocabulary.Within the scope of the claims the present invention can be made by regulation
Modification, and in without departing substantially from scope and spirit of the present invention, the present invention is revised.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, this
Bright can be extended to other all methods and applications with identical function.
Claims (10)
1. a kind of method preparing halogenation butyl rubber solution, it includes：
Butyl rubber slurry is passed through flash vaporization kettle by step i., hexane steam is passed through flash vaporization kettle simultaneously, and butyl rubber slurry is passed through
The charging position of flash vaporization kettle is higher than the charging position of hexane steam, and butyl rubber slurry is inversely connect in flash vaporization kettle with hexane steam
Touch and mass transfer, obtain the hexane solution containing butyl rubber；
The hexane solution obtaining in step i containing butyl rubber is passed directly into guide sieve-plate tower by step ii., in guide sieve-plate tower
Interior inversely contact with hexane steam, directly obtain the butyl rubber hexane solution for halogenation；The temperature of described guide sieve-plate tower
For 30-150 DEG C, pressure is 5-500KPa.
2. method according to claim 1 is it is characterised in that in the butyl rubber hexane solution that obtains in described step ii
Butyl rubber content is 10-20wt%.
3. method according to claim 1 is it is characterised in that in the butyl rubber hexane solution that obtains in described step ii
Unreacted monomer content is less than 1ppm.
4. the method according to any one in right 1-3 is it is characterised in that the operation temperature of described flash vaporization kettle is 30-70
DEG C, operating pressure is 0.1-0.5MPa.
5. the method according to any one in claim 1-3 is it is characterised in that the temperature of described guide sieve-plate tower is
50-90℃；Pressure is 20-200KPa.
6. in a kind of utilization claim 1-5, the method described in any one prepares the device of halogenation butyl rubber solution, bag
Include：
Flash vaporization kettle,
The guide sieve-plate tower being joined directly together with flash vaporization kettle；The temperature of described guide sieve-plate tower is 30-150 DEG C, and pressure is 5-
500KPa.
7. device according to claim 6 is it is characterised in that the butyl rubber that directly obtains from described linde sieve tray tower bottom
Glue hexane solution is directly used in halogenation.
8. device according to claim 6 is it is characterised in that directly obtain butyl rubber from described linde sieve tray tower bottom
In hexane solution, unreacted monomer content is less than 1ppm, and butyl rubber content is 10-20wt%.
9. the device according to any one in right 6-8 is it is characterised in that the operation temperature of described flash vaporization kettle is 30-70
DEG C, operating pressure is 0.1-0.5MPa.
10. the device according to any one in claim 6-8 is it is characterised in that the temperature of described guide sieve-plate tower is
50-90℃；Pressure is 20-200KPa.
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| CN109957056B (en) * | 2017-12-14 | 2021-07-02 | 中国石油化工股份有限公司 | Preparation method of halogenated monoolefin-conjugated diene copolymer |
| CN109535450B (en) * | 2018-11-20 | 2021-06-25 | 山东京博中聚新材料有限公司 | Butyl rubber solution, preparation method and preparation device thereof |
| CN109942841B (en) * | 2019-03-27 | 2021-10-26 | 山东京博中聚新材料有限公司 | Butyl rubber solution and preparation method thereof |
| CN112745516B (en) * | 2019-10-31 | 2022-07-12 | 中国石油化工股份有限公司 | Method and system for controlling concentration of feeding glue solution of glue solution refining tower |
| CN110938158B (en) * | 2019-12-18 | 2022-02-08 | 浙江信汇新材料股份有限公司 | Method and equipment for coagulating halogenated butyl rubber |
| CN111548436B (en) * | 2020-04-26 | 2021-04-16 | 浙江信汇新材料股份有限公司 | Preparation method of butyl rubber base rubber solution for halogenation reaction |
| CN114437256A (en) * | 2020-11-03 | 2022-05-06 | 北京诺维新材科技有限公司 | Preparation method and application of butyl rubber solution |
| CN114432721B (en) * | 2020-11-03 | 2023-09-15 | 北京诺维新材科技有限公司 | Polymer solution concentration method and application thereof |
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| RU2186788C1 (en) * | 2001-01-12 | 2002-08-10 | Открытое акционерное общество Научно-исследовательский институт "Ярсинтез" | Continuous butyl rubber halogenation process |
| CN102083868B (en) * | 2008-07-15 | 2013-06-19 | 朗盛国际股份公司 | Common solvent process for producing high molecular weight halobutyl rubber |
| CN103483483B (en) * | 2012-06-11 | 2015-09-09 | 中国石油化工集团公司 | A kind of isoprene-isobutylene rubber stripper plant and gas stripping process |
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2014
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